化工中间体三嗪环产业化工艺研究  

Study on Industrialization Process of Thiotriazinone

作　　者：于永宏 林琳 YU Yonghong;LIN in(Liaoning Medya Pharmaceutical Co.,Ltd.,Fushun Liaoning 113122,China)

机构地区：[1]辽宁美亚制药有限公司,辽宁抚顺113122

出　　处：《辽宁化工》2024年第4期555-558,共4页Liaoning Chemical Industry

摘　　要：目的:通过找出最佳工艺条件,提高产品质量和收率,利于产业化生产控制。方法:在混合溶剂中(一种极性质子溶剂和一种极性非质子溶剂)中,2-甲氨基硫脲、草酸二乙酯、甲醇钠在0~45℃缩合生成三嗪钠,然后经盐酸酸化得到目标产物三嗪环(TTZ)。结果:通过混合溶剂的使用,合成过程体系黏稠度得到大幅度改善,三嗪环(TTZ)收率提高到90%以上(以2-甲氨基硫脲计),纯度平均在99.5%以上,副产物1-甲基-5-巯基-1,2,4-三氮唑-3-羧酸甲酯(TTA)在0.1%以下。结论:该方法是合成三嗪环(TTZ)适宜的工业化方法。In order to improve the product quality and yield by finding out the optimal technological conditions,thiotriazinone sodium was synthesized by condensation of 2-methyl-3-thiosemicarbazide,diethyl oxalate and sodium methylate in a mixed solvent(a polar proton solvent and a polar non-proton solvent)at 0~45℃,then the target product thiotriazinone(TTZ)was obtained by hydrochloric acid acidification.By using mixed solvents,the viscosity of the synthesized process system was greatly improved,the yield of thiotriazinone(TTZ)was increased to more than 90%(calculated by 2-methyl-3-thiosemicarbazide),and the average purity was over 99.5%,the by-product material,1-methyl-5-mercapto-1,2,4-triazole-3-carboxylate(TTA),was less than 0.1%.So,this industrial method is suitable for the synthesis of thiotriazinone(TTZ).

关 键 词：中间体 三嗪环(TTZ) 合成 方法 

分 类 号：TQ463[化学工程—制药化工]